反应详情

To a mixture of 3-benzyloxy-N-methyl-2-nitroaniline (453.3 mg), 80% methanol (6.8 ml), anhydrous ferric chloride (13.6 mg) and carbon (13.6 mg) was dropwise added hydrazine monohydrate (255.6 μl), and the mixture was stirred for 5 hours at ambient temperature. Insoluble material was filtered off, and the filtrate was concentrated in vacuo. To the residue were added ethyl acetate and saturated sodium bicarbonate solution, and the separated organic layer was washed with water and brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by silica gel column chromatography (ethyl acetate—n-hexane) to give 2-amino-3-benzyloxy-N-methylaniline (348.9 mg).

1. filtrationInsoluble material was filtered off
2. concentrationthe filtrate was concentrated in vacuo
3. additionTo the residue were added ethyl acetate and saturated sodium bicarbonate solution
4. washthe separated organic layer was washed with water and brine
5. dry with materialdried over magnesium sulfate
6. customevaporated in vacuo
7. customThe residue was purified by silica gel column chromatography (ethyl acetate—n-hexane)